CN111732775A - Polymer composite material for space neutron shielding and preparation method thereof - Google Patents
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Abstract
The invention provides a polymer composite material for space neutron shielding and a preparation method thereof. The matrix of the composite material is polyethylene, and the filler of the composite material is spherical aluminum micron powder and graphene nanosheets with two-dimensional sheet structures. According to the invention, by utilizing the characteristics of high specific surface area and high conductivity of the graphene nanosheets, polyethylene is filled together with the aluminum micron powder, and the graphene nanosheets are uniformly distributed in the matrix to form a conductive percolation network, so that the conductivity of the composite material is improved; meanwhile, a large number of filler/matrix interfaces are created, neutron scattering is enhanced, neutron propagation paths are increased, and neutron shielding efficiency is improved; the prepared polyethylene composite material is convenient for secondary molding processing and can be installed and used on various electric and electronic devices of spacecrafts.
Description
[ technical field ] A method for producing a semiconductor device
The invention relates to the technical field of preparation and application of special composite materials in aerospace engineering, in particular to a polymer composite material for space neutron shielding and a preparation method thereof.
[ background of the invention ]
In the last two decades, in order to meet the actual requirements of aerospace engineering, particularly manned aerospace engineering, a great deal of research work is carried out at home and abroad to develop an anti-radiation composite material with the characteristics of light weight, high efficiency, structural function integration and the like. Recently, an effective shielding strategy and related materials are developed aiming at uncharged high-energy neutron irradiation in an aerospace environment, and wide attention is attracted. Because neutrons have the characteristics of heavy mass (equivalent to protons) and no electric charge, the neutrons have weak interaction with the atomic electron cloud of the material and extremely strong ability of penetrating the material; in addition, once the neutrons collide with the atomic nucleus of the material, stronger recoil atomic nucleus, proton and gamma ray can be generated, and stronger secondary radiation is caused. In the aerospace engineering, in order to ensure the physical health of astronauts and the normal operation of various devices of spacecrafts, high-energy neutrons must be effectively shielded. The shielding material adopted at present is aluminum alloy, but the specific gravity of the aluminum alloy is still larger, the neutron shielding efficiency is not high, and new materials which are lighter, higher in shielding efficiency and better in service performance need to be developed.
High molecular materials with high hydrogen content and low density are one of the candidates for high-energy neutron shielding materials. The main reason is that hydrogen has the most number of atomic nuclei per unit cross section, and can scatter more incident neutrons. Therefore, the polymer material is adopted as a matrix and is compounded with fillers with different chemical compositions and different structures to form composite materials with different functional characteristics, which is a research hotspot of the current neutron shielding materials. For example, CN103073773A, CN107652509A, CN103198871A, and CN110289115A respectively adopt carbon nanotubes, elemental boron powder, boron carbide powder, nano boron powder and other fillers to fill the polyethylene matrix, so as to obtain various composite materials with certain neutron shielding capability. Patent CN107880362A developed a silicone rubber with higher strength and neutron shielding performance by compounding carbon fibers and boride with silicone rubber. However, despite their lower density and better neutron shielding capabilities, most are electrically insulating and cannot replace the use of metallic conductors in spacecraft electronics. The novel composite material with good electric conduction capability, good neutron shielding performance and low density is developed, and the composite material has important application value in the aerospace field.
Accordingly, there is a need to develop a polymer composite for spatial neutron shielding and a method for preparing the same to address the deficiencies of the prior art to solve or mitigate one or more of the problems set forth above.
[ summary of the invention ]
In view of the above, the invention provides a polymer composite material for space neutron shielding and a preparation method thereof, wherein the composite material has good neutron shielding performance and high conductivity, and can shield neutron radiation in aerospace engineering.
In one aspect, the invention provides a polymer composite material for spatial neutron shielding, wherein a matrix of the composite material is polyethylene, and fillers of the composite material are aluminum micron powder and graphene nanosheets.
The above aspect and any possible implementation manner further provide an implementation manner, in the filler of the composite material, the aluminum micron powder is spherical, the graphene nanoplatelets are two-dimensional sheet structures, and the filler of the composite material is filled in the polyethylene matrix to form a conductive network.
The aspects and any possible implementations described above further provide an implementation where the aluminum micropowder has a mass fraction of [ 10%, 70% ], and the graphene nanoplatelets have a mass fraction of [ 0% to 3.5% ].
The above aspects and any possible implementations further provide an implementation where the aluminum micro powder has a particle size of 40-100 μm.
The above aspect and any possible implementation manner further provide an implementation manner, wherein the graphene nanoplatelets have a lateral dimension of 5-20 μm and a thickness of 1-2 nm.
The above aspects and any possible implementation manners further provide a preparation method of a polymer composite material for spatial neutron shielding, where the preparation method specifically includes:
adding required amounts of polyethylene matrix, aluminum micron powder and graphene nanosheets, or adding the polyethylene matrix and the aluminum micron powder into a high-speed mixer, mixing at the rotation speed of 100 plus one year at 1000rpm, adding into a screw extruder, and melting, mixing, extruding and granulating at the temperature of 170 plus one year at 250 ℃ to obtain the polymer composite material.
As described in the above aspect and any possible implementation manner, the preparation method of the graphene nanoplatelets specifically includes:
step 1: dialyzing the graphene oxide aqueous dispersion in high-purity water for 2 hours, and diluting to 0.05 wt% of concentration;
step 2: adding hydrazine hydrate, and controlling the mass ratio of the hydrazine hydrate to the graphene oxide to be 7: 10, adding ammonia water to adjust the pH value to 12;
and step 3: and carrying out reflux reaction for 4 hours at 95 ℃, filtering, washing, and freeze-drying to obtain the chemically reduced graphene nanosheet powder.
As for the above aspect and any possible implementation manner, there is further provided an implementation manner, when the addition amount of the graphene nanoplatelets is 0, the preparation method specifically includes: controlling the feeding mass ratio to ensure that the mass fraction of the aluminum micron powder is (10%, 70%), screening and drying the aluminum micron powder, physically stirring and mixing the aluminum micron powder with a polyethylene matrix, adding the mixture into a high-speed mixer, and mixing the aluminum micron powder and the polyethylene matrix at the rotation speed of 100 plus materials and 1000rpm to obtain a mixture; and finally, adding the mixture into a screw extruder, and carrying out melt mixing, extrusion and granulation at the temperature of 170-250 ℃ to obtain the polymer composite material, wherein the polymer composite material is an aluminum/polyethylene binary composite material.
As for the above aspect and any possible implementation manner, there is further provided an implementation manner, when the addition amount of the graphene nanoplatelets is not 0, the preparation method specifically includes: controlling the feeding mass ratio to ensure that the mass of the graphene nanosheets is (0%, 3.5%), physically stirring and mixing the graphene nanosheets, aluminum micron powder and polyethylene particles, adding the mixture into a high-speed mixer, mixing at the rotating speed of 100 plus materials at 1000rpm to obtain a mixture, finally adding the mixture into a screw extruder, and melting, mixing, extruding and granulating at the temperature of 170 plus materials at 250 ℃ to obtain a polymer composite material, wherein the polymer composite material is a polyethylene ternary composite material filled with aluminum powder and the graphene nanosheets together.
The above aspects and any possible implementation manners further provide an implementation manner, in which the polymer composite material is subjected to hot press molding at 220 ℃ and 150 ℃ to obtain an article meeting the dimensional requirement, and a performance test is performed, where the performance test includes: observing the section morphology of the sample wafer by using a scanning electron microscope, testing the neutron transmittance of the sample wafer by using a neutron diffraction spectrometer, and testing the room-temperature conductivity of the sample wafer by using a resistivity tester.
Compared with the prior art, the invention can obtain the following technical effects:
1. according to the invention, by utilizing the characteristics of high specific surface area and high conductivity of the graphene nanosheets, polyethylene is filled together with the aluminum micron powder, and the graphene nanosheets are uniformly distributed in the matrix to form a conductive percolation network, so that the conductivity of the composite material is improved; meanwhile, a large number of filler/matrix interfaces are created, neutron scattering is enhanced, neutron propagation paths are increased, and neutron shielding efficiency is improved;
2. the invention has the characteristics of low equipment cost, simple process and the like, and the prepared polyethylene composite material is convenient for secondary forming processing and can be installed and used on various spacecraft electrical and electronic equipment.
Of course, it is not necessary for any one product in which the invention is practiced to achieve all of the above-described technical effects simultaneously.
[ description of the drawings ]
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without creative efforts.
Fig. 1 is a scanning electron micrograph of a cross section of a ternary composite material formed by polyethylene filled with aluminum microspheres and graphene nano-sheets according to an embodiment of the present invention.
[ detailed description ] embodiments
For better understanding of the technical solutions of the present invention, the following detailed descriptions of the embodiments of the present invention are provided with reference to the accompanying drawings.
It should be understood that the described embodiments are only some embodiments of the invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The terminology used in the embodiments of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used in the examples of the present invention and the appended claims, the singular forms "a," "an," and "the" are intended to include the plural forms as well, unless the context clearly indicates otherwise.
The invention provides a polymer composite material for space neutron shielding, wherein a matrix of the composite material is polyethylene, a filler is spherical aluminum micron powder and a graphene nanosheet with a two-dimensional sheet structure, the mass fraction of the aluminum micron powder is more than or equal to 10% and less than or equal to 70%, and the mass fraction of the graphene nanosheet is more than or equal to 0% and less than or equal to 3.5%: the average grain diameter of the aluminum micron powder is 60 microns: the graphene nanosheet is obtained by reducing and oxidizing the graphene nanosheet through hydrazine hydrate, washing, freeze drying and the like, and is 5-20 microns in transverse size and about 1-2nm in thickness.
The invention also provides a preparation method of the composite material of the polymer composite material for space neutron shielding, which comprises the following steps:
s1: adding a polyethylene matrix, aluminum micron powder and graphene nanosheets into a high-speed mixer, and mixing at the rotation speed of 100-1000rpm to obtain a mixture;
s2: adding the mixture into a screw extruder, and carrying out melt mixing, extrusion and granulation at the temperature of 170-250 ℃ to obtain a composite material;
s3: and carrying out hot-press molding on the obtained composite material granules at the temperature of 150-220 ℃ to obtain the product with the required size.
The technical scheme of the invention is as follows:
(1) the matrix of the prepared composite material is polyethylene, and the filler is aluminum micron powder with a spherical structure and graphene nanosheets with a two-dimensional sheet structure. The aluminum micron powder and the graphene nanosheets are jointly filled in the polyethylene matrix, and the aluminum micron powder and the graphene nanosheets cooperatively form a conductive network, so that the composite material is endowed with excellent electric conduction capability. Meanwhile, the graphene nanosheets are introduced to assist the aluminum micron powder to form uniform and stable dispersion in the polyethylene matrix.
(2) The average particle size of the aluminum micropowder used is about 60 microns.
(3) The two-dimensional graphene nanosheet is prepared from graphene oxide serving as a raw material by liquid-phase-assisted ultrasonic stripping, hydrazine hydrate chemical reduction, washing and freeze drying to obtain dry powder, wherein the transverse size of the dry powder is about 5-20 microns, and the thickness of the dry powder is about 1-2 nm.
(4) And adding the obtained two-dimensional graphene nanosheet dry powder, aluminum micron powder and a polyethylene matrix into a high-speed mixer together to obtain a mixture.
(5) And (4) adding the mixture obtained in the step (4) into a screw extruder for melting, mixing, granulating and finally performing hot-press molding to obtain a composite material sample.
The key point of the invention is that the characteristics of high specific surface area and high conductivity of the graphene nanosheets are utilized, the graphene nanosheets and the aluminum micron powder are filled with polyethylene and uniformly distributed in the matrix to form a conductive percolation network, so that the conductivity of the composite material is improved; meanwhile, a large number of filler/matrix interfaces are created, neutron scattering is enhanced, neutron propagation paths are increased, and neutron shielding effect is improved.
Example 1
Sieving a certain amount of aluminum micron powder, and drying. Physically stirring and mixing with a certain amount of polyethylene matrix, adding into a high-speed mixer, and mixing at the rotation speed of 100-1000rpm to obtain a mixture; and finally, adding the mixture into a screw extruder, and carrying out melt mixing, extrusion and granulation at the temperature of 170-250 ℃ to obtain the aluminum/polyethylene binary composite material. The feeding mass ratio is controlled to ensure that the mass fraction of the aluminum micron powder is between 10 and 70 percent.
Example 2
The graphene oxide aqueous dispersion was dialyzed in high-purity water for 2 hours and diluted to a concentration of 0.05 wt%. Adding hydrazine hydrate, and controlling the mass ratio of the hydrazine hydrate to the graphene oxide to be 7: and 10, adding ammonia water to adjust the pH value to 12, carrying out reflux reaction for 4 hours at the temperature of 95 ℃, and filtering, washing, freezing and drying to obtain chemically reduced graphene nanosheet powder.
Example 3
Physically stirring and mixing the graphene nanosheet prepared by the method in the embodiment 2, the aluminum micron powder and a certain amount of polyethylene particles, adding the mixture into a high-speed mixer, and mixing at the rotation speed of 100-1000rpm to obtain a mixture; and finally, adding the mixture into a screw extruder, and carrying out melt mixing, extrusion and granulation at the temperature of 170-250 ℃ to obtain the polyethylene ternary composite material filled with the aluminum powder and the graphene nanosheets. And controlling the feeding mass ratio to ensure that the mass fraction of the aluminum micron powder is 60 percent and the mass of the graphene nano sheet is 0-3.5 percent.
Example 4
And carrying out hot-press molding on the master batch of the composite material containing the aluminum powder and the graphene nanosheets with different mass fractions to obtain a sheet. And controlling the thickness of the die, the processing temperature and the pressure to obtain a sample wafer with the thickness of 0.5 mm. And observing the section morphology of the sample by using a scanning electron microscope. And testing the neutron transmittance of the sample by using a neutron diffraction spectrometer. And testing the room-temperature conductivity of the sample wafer by using a resistivity tester.
Fig. 1 is a scanning electron micrograph of a cross section of a ternary composite material formed by filling polyethylene with aluminum microspheres and graphene nanosheets, wherein the mass fraction of the aluminum microspheres is 60% and the mass fraction of the graphene nanosheets is 3.5%.
The specific performance test results are shown below, and table 1 shows the formulation, conductivity and neutron shielding performance of the composite material prepared according to the technical route of the present invention.
TABLE 1
As can be seen from table 1, filler content has a significant effect on neutron transmission and electrical conductivity of the resulting composite. The neutron transmittance of a composite material sample with the thickness of 0.5mm can be reduced from 72% to 64% by changing the content of the binary filler, and the conductivity can be regulated and controlled within two magnitude ranges of 1-100S/m. Meanwhile, in order to improve neutron shielding efficiency, a composite material with a larger thickness can be adopted. The data in table 1 show that the fixed aluminum micron powder (mass fraction of 60%) and graphene nanoplatelets (mass fraction of 3.5%) are unchanged, the thickness of the coupon increases from 0.5mm to 2.0mm, and the neutron transmittance decreases from 64% to 13.5%.
The requirements on the density, the conductivity and the neutron shielding efficiency of the composite material are comprehensively considered, and the preferred technical scheme is that the ternary composite material is prepared from 60% and 3.5% of aluminum micron powder and 3.5% of graphene nanosheet in mass fraction respectively.
The composite materials provided in the examples of the present application are described in detail above. The above description of the embodiments is only for the purpose of helping to understand the method of the present application and its core ideas; meanwhile, for a person skilled in the art, according to the idea of the present application, there may be variations in the specific embodiments and the application scope, and in summary, the content of the present specification should not be construed as a limitation to the present application.
As used in the specification and claims, certain terms are used to refer to particular components. As one skilled in the art will appreciate, manufacturers may refer to a component by different names. This specification and claims do not intend to distinguish between components that differ in name but not function. In the following description and in the claims, the terms "include" and "comprise" are used in an open-ended fashion, and thus should be interpreted to mean "include, but not limited to. "substantially" means within an acceptable error range, and a person skilled in the art can solve the technical problem within a certain error range to substantially achieve the technical effect. The description which follows is a preferred embodiment of the present application, but is made for the purpose of illustrating the general principles of the application and not for the purpose of limiting the scope of the application. The protection scope of the present application shall be subject to the definitions of the appended claims.
It is also noted that the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a good or system that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such good or system. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other like elements in a commodity or system that includes the element.
It should be understood that the term "and/or" as used herein is merely one type of association that describes an associated object, meaning that three relationships may exist, e.g., a and/or B may mean: a exists alone, A and B exist simultaneously, and B exists alone. In addition, the character "/" herein generally indicates that the former and latter related objects are in an "or" relationship.
The foregoing description shows and describes several preferred embodiments of the present application, but as aforementioned, it is to be understood that the application is not limited to the forms disclosed herein, but is not to be construed as excluding other embodiments and is capable of use in various other combinations, modifications, and environments and is capable of changes within the scope of the application as described herein, commensurate with the above teachings, or the skill or knowledge of the relevant art. And that modifications and variations may be effected by those skilled in the art without departing from the spirit and scope of the application, which is to be protected by the claims appended hereto.
Claims (10)
1. The polymer composite material for spatial neutron shielding is characterized in that a matrix of the composite material is polyethylene, and a filler of the composite material comprises aluminum micron powder and graphene nanosheets.
2. The composite material according to claim 1, wherein the aluminum micron powder in the filler of the composite material is spherical, the graphene nanosheets are in a two-dimensional sheet structure, and the filler of the composite material is filled in a polyethylene matrix to form a conductive network.
3. The composite material according to claim 1, wherein the composite material has a mass fraction of aluminum micropowder of [ 10%, 70% ], a mass fraction of graphene nanoplatelets of [ 0%, 3.5% ], and a polyethylene matrix remaining.
4. The composite material according to claim 1, characterized in that the aluminium micropowders have a particle size of 40-100 μm.
5. The composite material of claim 1, wherein the graphene nanoplatelets have a lateral dimension of 5-20 μ ι η and a thickness of 1-2 nm.
6. A preparation method of a polymer composite material for space neutron shielding is characterized by comprising the following specific steps:
adding required amounts of polyethylene matrix, aluminum micron powder and graphene nanosheets, or adding the polyethylene matrix and the aluminum micron powder into a high-speed mixer, mixing at the rotation speed of 100 plus one year at 1000rpm, adding into a screw extruder, and melting, mixing, extruding and granulating at the temperature of 170 plus one year at 250 ℃ to obtain the polymer composite material.
7. The preparation method according to claim 6, wherein the preparation method of the graphene nanoplatelets is specifically as follows:
step 1: dialyzing the graphene oxide aqueous dispersion in high-purity water for 2 hours, and diluting to 0.05 wt% of concentration;
step 2: adding hydrazine hydrate, and controlling the mass ratio of the hydrazine hydrate to the graphene oxide to be 7: 10, adding ammonia water to adjust the pH value to 12;
and step 3: and carrying out reflux reaction for 4 hours at 95 ℃, filtering, washing, and freeze-drying to obtain the chemically reduced graphene nanosheet.
8. The preparation method according to claim 6, wherein when the addition amount of the graphene nanoplatelets is 0, the preparation method specifically comprises the following steps: controlling the feeding mass ratio to ensure that the mass fraction of the aluminum micron powder is between 10 and 70 percent, screening and drying the aluminum micron powder, physically stirring and mixing the aluminum micron powder with a polyethylene matrix, adding the mixture into a high-speed mixer, and mixing the aluminum micron powder and the polyethylene matrix at the rotation speed of 100 plus materials and 1000rpm to obtain a mixture; and finally, adding the mixture into a screw extruder, and carrying out melt mixing, extrusion and granulation at the temperature of 170-250 ℃ to obtain the polymer composite material, wherein the polymer composite material is an aluminum/polyethylene binary composite material.
9. The preparation method according to claim 7, wherein when the addition amount of the graphene nanoplatelets is not 0, the preparation method specifically comprises: controlling the feeding mass ratio to ensure that the mass of the graphene nanosheets is (0% -3.5%), physically stirring and mixing the graphene nanosheets, aluminum micron powder and polyethylene particles, adding the mixture into a high-speed mixer, mixing at the rotating speed of 100 plus materials at 1000rpm to obtain a mixture, finally adding the mixture into a screw extruder, and melting, mixing, extruding and granulating at the temperature of 170 plus materials at 250 ℃ to obtain a polymer composite material, wherein the polymer composite material is a polyethylene ternary composite material filled with aluminum powder and the graphene nanosheets together.
10. The preparation method of claim 6, wherein the polymer composite is hot-pressed and molded at the temperature of 150 ℃ and 220 ℃ to obtain a product meeting the dimensional requirement and to perform a performance test, wherein the performance test comprises: observing the section morphology of the sample wafer by using a scanning electron microscope, testing the neutron transmittance of the sample wafer by using a neutron diffraction spectrometer, and testing the room-temperature conductivity of the sample wafer by using a resistivity tester.
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